The morphology of anodic aluminum oxide films formed in neutral aqueous 3% ammonium tartrate was investigated using transmission and replica electron microscopy and transmission stereoscopy. After an initiation period of approximately 90 min, corresponding to the appearance of a minimum in the potentiostatic anodic current, development of a porous structure was observed. The film structure was comparable to that formed in conventional pore-forming electrolytes at shorter times, with approximately polygonal oxide cells, each containing a central pore. Pore depth and diameter both increased in a systematic manner with anodizing time; a hypothetical model relying on fieldassisted dissolution of oxide, with local field enhancement due to the pore geometry, is used to explain this dependence. At longer times, the pore depth increases linearly with anodizing time, also consistent with this model and with the observed establishment of a stable pore structure. The stable pore size and oxide cell size are proportional to formation voltage in accord with the geometric argument forwarded to explain pore coalescence and the formation of stable terminal pores.Anodic aluminum oxide films are commonly classified as porous or barrier-type (i.e., nonporous) according to the electrolyte in which they are formed. Barrier-type films are formed by anodically polarizing aluminum in an electrolyte which exerts little solvent action on the oxide film, e.g., aqueous borate or tar-* Electrochemical Society Active Member. ) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 138.251.14.35 Downloaded on 2015-05-23 to IP ) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 138.251.14.35 Downloaded on 2015-05-23 to IP ) unless CC License in place (see abstract). ecsdl.org/site/terms_use address. Redistribution subject to ECS terms of use (see 138.251.14.35 Downloaded on 2015-05-23 to IP
Anodized specimens of aluminum and tantalum were deformed in laboratory air; strain to failure and the failure characteristics of the oxide film were evaluated optically. Barrier-type anodie aluminum oxide films of thickness greater than N400A failed at ~0.925% strain normal to the tensile axis and apparently suppressed substrate slip emergence. Thinner anodic films on aluminum failed along substrate slip traces at ~1.12% strain. These films did not suppress slip emergence, but were apparently stronger. The presence of a porous oxide superimposed on thin barrier-type films caused them to fail in the thick film mode; this was the only effect of a porous layer. Anodic films on mechanically polished tantalum failed at N0.28% strain, independent of thickness, but showed a failure mode dependence on thickness analogous to that of aluminum. Films on chemically polished tantalum substrates always failed in simple tension, but showed a thickness dependence, failing at ~0.14% strain for thicknesses greater than ~680A, and ~0.20% strain for thicknesses less than that value. Failure of these films was accompanied by separation of the films from the substrate.Environment-sensitive failure processes such as stress corrosion crackir~g and corrosion fatigue involve a complex interplay of chemical and mechanical aggression and are far from well understood. Oxide film failure is seen by many investigators as a necessary prelude to the initiation and propagation of cracks in these processes (1-7). The literature dealing with the mechanical behavior of oxide films is not voluminous, and reported values of mechanical properties, e.g., Young's modulus, film strength, and film failure strain, exhibit large variations. Edeleanu and Law (8) strained thick porous anodic films on aluminum in tension and found them to be elastic, with failure occurring at 1-2% strain normal to the tensile axis. Bradhurst and Leach (9, 10) deformed aluminum specimens bearing barrier-type anodic films, detecting film failure by a variety of electrical methods to occur at 1-3% strain. For 1500A films removed from the substrate, a failure strain of 2.48% and a Young's modulus of ~ 41 • 1,08 MN/m 2 were determined. Also using electrical detection methods, Bubar and Vermilyea (11, 12) found thin anodic films on aluminum to exhibit some ductility, while thick films were brittle. They also observed a large ductility, as much as 50% elongation prior to fracture, in anodic tantalum oxide films tested in this wet manner, in marked contrast to the value of 0.83% reported by Eliezer and Brandon (13), who used a (dry) bulge test technique. In earlier work Young (14) had attributed this discrepancy to the presence of a surface film on chemically polished specimens. This film gave rise to poor adhesion of the anodic oxide, with consequent oxide detachment and brittle behavior, whereas removal of this "preanodic" film by leaching in boiling water resulted in a very adherent, ductile anodic oxide. Grosskreutz (15,16) found anodic aluminum oxide films, both adherent to and s...
Die Porengeometrie anodischer in neutraler (pH 7) 30%iger wäßriger NH4‐tartratlösung (potentiostatisch) gebildeter Al‐oxidfilme wird mit Hilfe der Transmissions‐ und Abdruckelektronenmikroskopie sowie der Transmissionsstereoskopie in Abhängigkeit von Anodisierungszeit (bis zu 48 h) und Bildungspotential untersucht.
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